ImageVerifierCode 换一换
格式:PDF , 页数:14 ,大小:965.75KB ,
资源ID:715797      下载积分:10000 积分
快捷下载
登录下载
邮箱/手机:
温馨提示:
如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
如填写123,账号就是123,密码也是123。
特别说明:
请自助下载,系统不会自动发送文件的哦; 如果您已付费,想二次下载,请登录后访问:我的下载记录
支付方式: 支付宝扫码支付 微信扫码支付   
注意:如需开发票,请勿充值!
验证码:   换一换

加入VIP,免费下载
 

温馨提示:由于个人手机设置不同,如果发现不能下载,请复制以下地址【http://www.mydoc123.com/d-715797.html】到电脑端继续下载(重复下载不扣费)。

已注册用户请登录:
账号:
密码:
验证码:   换一换
  忘记密码?
三方登录: 微信登录  

下载须知

1: 本站所有资源如无特殊说明,都需要本地电脑安装OFFICE2007和PDF阅读器。
2: 试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。
3: 文件的所有权益归上传用户所有。
4. 未经权益所有人同意不得将文件中的内容挪作商业或盈利用途。
5. 本站仅提供交流平台,并不能对任何下载内容负责。
6. 下载文件中如有侵权或不适当内容,请与我们联系,我们立即纠正。
7. 本站不保证下载资源的准确性、安全性和完整性, 同时也不承担用户因使用这些下载资源对自己和他人造成任何形式的伤害或损失。

版权提示 | 免责声明

本文(EN 16343-2013 en Cosmetics - Analysis of cosmetic products - Determination of 3-iodo-2-propynyl butylcarbamate (IPBC) in cosmetic preparations LC-MS methods《化妆品 化妆品分析 化妆品备制中碘代丙炔基正丁.pdf)为本站会员(tireattitude366)主动上传,麦多课文库仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文库(发送邮件至master@mydoc123.com或直接QQ联系客服),我们立即给予删除!

EN 16343-2013 en Cosmetics - Analysis of cosmetic products - Determination of 3-iodo-2-propynyl butylcarbamate (IPBC) in cosmetic preparations LC-MS methods《化妆品 化妆品分析 化妆品备制中碘代丙炔基正丁.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16343:2013Cosmetics Analysisof cosmetic products Determination of 3-iodo-2-propynyl butylcarbamate (IPBC)in cosmetic preparations, LC-MS methodsBS EN 16343:2013 BRITISH STA

2、NDARDNational forewordThis British Standard is the UK implementation of EN 16343:2013.The UK participation in its preparation was entrusted to TechnicalCommittee CW/217, Cosmetics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does n

3、ot purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 76543 8ICS 71.100.70Compliance with a British Standard cannot confer immunity fromlegal obli

4、gations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 May 2013.Amendments issued since publicationDate Text affectedBS EN 16343:2013EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16343 May 2013 ICS 71.100.70 English Version Cosmetic

5、s - Analysis of cosmetic products - Determination of 3-iodo-2-propynyl butylcarbamate (IPBC) in cosmetic preparations, LC-MS methods Cosmtiques - Analyse des produits cosmtiques - Dtermination quantitative du carbamate 3-iodo-2-propynylbutyle (IPBC), mthodes CL-SM Kosmetische Mittel - Untersuchung v

6、on kosmetischen Mitteln - Bestimmung von 3-Iod-2-propinylbutylcarbamat (IPBC) in kosmetischen Mitteln, LC-MS-Verfahren This European Standard was approved by CEN on 25 April 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

7、 European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official ve

8、rsions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austri

9、a, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,

10、 Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Memb

11、ers. Ref. No. EN 16343:2013: EBS EN 16343:2013EN 16343:2013 (E) 2 Contents Page Foreword . 3 1 Scope 4 2 Principle 4 3 Reagents . 4 4 Apparatus and equipment . 5 5 Procedure . 5 6 Evaluation . 7 7 Test report 7 Annex A (informative) Results of the inter-laboratory test . 8 Bibliography 9 BS EN 16343

12、:2013EN 16343:2013 (E) 3 Foreword This document (EN 16343:2013) has been prepared by Technical Committee CEN/TC 392 “Cosmetics”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endors

13、ement, at the latest by November 2013, and conflicting national standards shall be withdrawn at the latest by November 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for iden

14、tifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugo

15、slav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16343:2013EN 16343:2013 (E) 4 1 Scope This

16、 European Standard specifies a method for the quantitative determination of 3-iodo-2-propynyl butylcarbamate (IPBC) in the concentration range from 0,005 g/100 g to 0,1 g/100 g - Annex V No. 56 in Regulation (EC) No 1223/2009 on cosmetic products. 2 Principle IPBC is extracted from the cosmetic prep

17、aration using methanol. IPBC present in the sample extract is separated using reverse phase HPLC with mass specific detection (LC-MS or LC-MS/MS). Quantitative determination of IPBC is made using the external standard method of calibration or standard addition. 3 Reagents 3.1 General If not otherwis

18、e specified, analytical-grade chemicals shall be used; water shall be distilled or of a suitable purity. “Solution” shall be understood as an aqueous solution unless otherwise specified. 3.2 Iodopropynyl butylcarbamat, CAS number: 55406-53-6 (Supplier : Sigma-Aldrich1)(521949), Dr. Ehrenstorfer GmbH

19、1)(C 14335000). 3.3 Methanol, HPLC grade, CAS number: 67-56-1. 3.4 Formic acid, CAS number: 64-18-6. 3.5 Tetrahydrofuran (THF), CAS number: 109-99-9. 3.6 Propan-2-ol, CAS number: 67-63-0. 3.7 Eluents 3.7.1 Eluent A, 1 ml of formic acid (3.4) is mixed with 1 000 ml of water. 3.7.2 Eluent B, Methanol

20、(3.3). 3.8 IPBC stock solution, = 1 mg/ml. Weigh approximately 0,05 g of IPBC (3.2) into a 50-ml-volumetric flask. Firstly, dissolve in a small amount of methanol (3.3) and then fill up to the calibration mark with methanol. This solution has a shelf life of 8 weeks if it is stored in a refrigerator

21、. 3.9 Calibration solutions (standard solutions) 5,0 ml of the stock solution (3.8) is transferred into a 50-ml-volumetric flask and filled to the calibration mark with methanol (3.3), ( = 0,1 mg/ml or 100 g/ml). From this solution, at least 5 solutions are prepared by dilution to obtain IPBC concen

22、trations of = 0,05 g/ml to = 1,0 g/ml. These solutions have a shelf life of 8 weeks if they are stored in a cool place. Examples of dilutions are given in Table 1. 1) This is an example of a suitable product available commercially. This information is given for the convenience of users of this docum

23、ent and does not constitute an endorsement by CEN of this product. Equivalent products may be used if they can be shown to lead to the same results. BS EN 16343:2013EN 16343:2013 (E) 5 Table 1 Calibration solutions No. Preparation Dilution Concentration g/ml 3.9 5 ml 3.8 filled up to 50 ml 1:10 100

24、3.10 10 ml 3.9 filled up to 100 ml 1:100 10 3.11 10 ml 3.10 filled up to 100 ml 1:1000 1 3.12 4 ml 3.10 filled up to 50 ml 1:1250 0,8 3.13 5 ml 3.10 filled up to 100 ml 1:2000 0,5 3.14 10 ml 3.11 filled up to 50 ml 1:5000 0,2 3.15 5 ml 3.11 filled up to 50 ml 1:10000 0,1 4 Apparatus and equipment 4.

25、1 Standard laboratory equipment 4.2 Membrane filter, in the form of a disposable syringe filter, pore width: 0,2 m2). 4.3 High-performance liquid chromatograph, suitable for gradient elution with mass-specific detector. 4.4 Analytical separation column, the following parameters have proved useful: R

26、P 18 Phase, 5 m, 150 mm 2 mm, e.g. Zorbax1), Spherisorb1), Phenomenex-Luna1)or equivalent. If a precolumn is used, it shall have the same analytical properties as the separation column. 5 Procedure 5.1 Sample preparation Weigh approximately 200 mg of the sample to the nearest 0,1 mg into a 20-ml-vol

27、umetric flask (alternatively a 50-ml-volumetric flask). Add 1,5 ml of THF (3.5) and shake. Add 10 ml of methanol (3.3), and allow to dissolve or suspend for 5 min in the ultrasonic bath at room temperature. Allow to cool to room temperature and fill to the calibration mark with methanol (3.3). The s

28、ample solution is diluted with methanol (3.3) to a ratio of 1:10, filtered through a membrane filter (4.2) and then analysed using LC-MS or LC-MS/MS. For poorly soluble or suspendable matrices it is recommended to partially dissolve the sample by adding 2 ml of 2-propanol (3.6) instead of THF (3.5)

29、or to stir it with a magnetic stirrer for 30 min prior to the treatment in the ultrasonic bath. 5.2 Liquid chromatography (LC) conditions When using the apparatus (4.3) and column (4.4), the following conditions have shown to be useful (see Table 2): 2) The ring test was performed using 0,2 m filter

30、. BS EN 16343:2013EN 16343:2013 (E) 6 Table 2 Gradient programme Time min Fraction eluent A % Fraction eluent B % 0 85 15 8 10 90 12 10 90 13 85 15 25 85 15 Column: RP 18 Phase, 5 m, 150 mm 2 mm Injection volume: 1 l to 10 l Flow rate: 0,2 ml/min Column oven temperature: 25 C 5.3 Detection 5.3.1 Gen

31、eral The detection and quantitative determination can be performed by evaluating the mass traces of IPBC or by evaluating the fragment ions. To avoid false low results by adduct formation occurring in the MRM mode of the Electrospray (ESI) method, the APCI (Atmospheric Pressure Chemical Ionisation)

32、method should be used for ionisation. 5.3.2 MS detection in Selected Ion Monitoring (SIM) mode Mass traces: m/z 282 M+H+and m/z 304 M+Na+. Evaluation is based on the total ion current (from the sum of the two masses). 5.3.3 MS detection in Multiple Reaction Monitoring (MRM) mode Protonated molecule

33、ion: 282 M+H+Fragment ion 1: 57 Fragment ion 2: 165 Evaluation is based on the most sensitive fragment ion. Since the analyte may form adducts with sodium ions, false low results can be obtained if larger amounts of sodium ions are present in the sample. If ESI ionisation is used, standard addition

34、should therefore be performed using the MRM mode so as to ensure reliable quantification results. When performing the standard addition, the content of the added IPBC should not exceed the content expected in the sample. BS EN 16343:2013EN 16343:2013 (E) 7 6 Evaluation 6.1 Identification and quantit

35、ative determination The IPBC is identified by comparing the retention times of the sample with those of calibration solutions. The quantitative determination of the analyte is performed based on a calibration function or the standard addition. The calibration solutions are chromatographed in accorda

36、nce with the conditions given in 5.2. The IPBC concentration is calculated from the calibration by linear regression on the basis of the obtained peak area. 6.2 Calculation The preservative content w in g/100 g, with respect to the sample, is calculated using the following formula: 10001000100=mFVcw

37、 (1) where w is the IPBC content, in g/100 g; c is the IPBC concentration in the sample solution, in g/ml, determined from the calibration function; m is the initial weight of the sample, in g; V is the volume of the sample measurement solution, in ml; F is the dilution factor, if required. The resu

38、lt is given in g/100 g, rounded to three decimal places. 7 Test report The test report shall contain the following data: a) information necessary for the identification of the sample (type, origin and designation of the sample); b) a reference to this European Standard; c) name of the laboratory per

39、forming the test; d) the date and type of sampling procedure (if known); e) the date of receipt and date of analysis; f) the date of test; g) the test results and the units in which they have been expressed; h) justification of any deviations from this official method; i) operations not specified in

40、 the method or regarded as optional, which might have affected the results. BS EN 16343:2013EN 16343:2013 (E) 8 Annex A (informative) Results of the inter-laboratory test This method has been developed by the working group “Cosmetics” of the German Federal Office of Consumer Protection and Food Safe

41、ty (BVL) for the purpose of implementing Section 64 of the Food and Feed Code (LFGB). It has been tested in an inter-laboratory test with a total of 13 participants. The following statistical data presented in Table A.1 have been determined for shower gel and cream in an inter-laboratory test with 1

42、3 participating laboratories using external quantification. Table A.1 Statistical data of the inter-laboratory test Parameter LC-MS method IPBC content, in g/100 g Shower gel Cream Number of participating laboratories 13 13 Number of outliers 3 2 Number of laboratories after elimination of the outli

43、ers 10 11 Mean value x , g/100 g 0,013 0,019 Repeatability r, g/100 g 0,003 0,003 Repeatability standard deviation sr, g/100 g 0,001 0,001 Reproducibility R, g/100 g 0,006 0,005 Reproducibility standard deviation sR, g/100 g 0,002 0,002 Recovery, % 101,4 103,7 BS EN 16343:2013EN 16343:2013 (E) 9 Bib

44、liography 1 Frauen M, Steinhart H, Rapp C, Hintze U. (2001): Rapid quantification of iodopropynyl butylcarbamate as the preservative in cosmetic formulations using high-performance liquid chromatography-electrospray mass spectrometry. J Pharm Biomed Anal. 25 (5-6):965-70 This page deliberately left

45、blankThis page deliberately left blankBSI is the independent national body responsible for preparing British Standards and other standards-related publications, information and services. It presents the UK view on standards in Europe and at the international level. BSI is incorporated by Royal Chart

46、er. British Standards and other standardisation products are published by BSI Standards Limited.British Standards Institution (BSI)raising standards worldwideBSI389 Chiswick High Road London W4 4AL UKTel +44 (0)20 8996 9001Fax +44 (0)20 8996 Standards and PASs are periodically updated by amendment

47、or revision. Users of British Standards and PASs should make sure that they possess the latest amendments or editions.It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using British Standards wou

48、ld inform the Secretary of the technical committee responsible, the identity of which can be found on the inside frontcover. Similary for PASs, please notify BSI Customer Services.Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001BSI offers BSI Subscribing Members an individual updating service calle

49、d PLUS which ensures that subscribers automatically receive the latest editions of British Standards and PASs.Tel: +44 (0)20 8996 7669 Fax: +44 (0)20 8996 7001Email: Buying standardsYou may buy PDF and hard copy versions of standards directly using acredit card from the BSI Shop on the website addition all orders for BSI, international and foreign standards publicationscan be addressed to BSI Customer Services.Tel: +44 (0)20 8996 9001 Fax: +44

copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
备案/许可证编号:苏ICP备17064731号-1